A kind of preparation method of the graphene microchip composite printed for 3D
Technical field
The present invention relates to grapheme material field, be specifically related to the preparation method of a kind of graphene microchip composite printed for 3D.
Background technology
Graphene is the another Novel Carbon Nanomaterials being found after CNT, it it is the two-dimentional carbon film of a kind of only one of which atomic thickness, be people find so far a kind of by the material of individual layer atomic building, carbon film is connected into hexagonal network by chemical bond between carbon atom, owing to the chemical bond between carbon atom is made up of sp2 hybridized orbit, therefore Graphene is the most indomitable, possessing the good characteristic that other new materials such as bent, electric conductivity is strong, mechanical strength good, light transmission is good do not possess, these characteristics make the preparation method of Graphene receive much concern all the time.
Graphite, because natively having the bedded structure that can peel off, therefore can carry out peeling off acquisition Graphene by graphite carries out the Strong shear of machinery.The most generally use the strong mechanical shearing of the method such as ball milling, mortar to prepare Graphene.As Chinese invention patent application number 201510073825.0 discloses a kind of tonne of class mechanical stripping device producing Graphene and production method thereof, it is by rotor as a mill, when rotor rotates, the outer surface of rotor and the internal grinding of material bin, so that graphite is stripped thinning acquisition Graphene.Owing to being difficult to separate the Graphene peeled off in time in the process of lapping of strength, easily cause reunion.Therefore, the Graphene obtained in mechanical grinding process, owing to reaching Nano grade, is the most easily reunited and overlapping, so that the Rotating fields hydraulic performance decline of Graphene.Thus affect the commercial application of grapheme material powder.
In order to realize quickly peeling off Graphene, grapheme material powder can also be prepared by oxidation-reduction method, but when preparing grapheme material powder by this kind of method, purpose is crystalline flake graphite deep oxidation, connect various oxy radical equably at graphite flake layer and support the interlamellar spacing of big graphite, then ultrasonic equipment easily peels away graphite flake layer, finally produces Graphene plus chemical substance reduction.But the Graphene that such method is worked it out, strong oxidizing process can cause a large amount of defects of graphene-structured, and these defects cause the significantly decline of Graphene performance.The Graphene additionally aoxidized can not be repaired even across reduction, the defect of the lamellar structure of graphite.
Even if using said method mechanical stripping and redox to obtain Graphene, owing to still there being strong Van der Waals force between graphene sheet layer, the when of being dried or during aft-loaded airfoil, it is easy to secondary between lamella overlapping, thus balances out effect of physics stripping process.Therefore, Graphene is difficult to after being difficult to volume production and reaching nano-scale disperse the defects such as storage to make the application of Graphene by the most hindered.
In consideration of it, graphene microchip is to solve the optimal selection of Graphene application.Graphene microchip is a kind grapheme material, and its lamella average thickness is within 15nm, and does not meets the definition of the Graphene less than 10 layers of strict demand.But remain the mechanical strength of excellence, conduction, heat conductivility.Present invention seek to address that mass production and the dispersive property of graphene microchip, to reach the application in 3D prints.
Summary of the invention
Being difficult to scattered defect, and the layer of the Graphene the most overlapping defect assembled for the application in 3D prints of current Graphene, the present invention proposes the preparation method of a kind of graphene microchip composite printed for 3D.Graphite heating is first disperseed by the method, the blade driven by the rotor of Type Impact Superfine Mill carries out shearing repeatedly, impact to graphite, graphite linings is made to peel off, after classified screening, qualified material after electrostatic dispersion, be uniformly dispersed, good fluidity for 3D print graphene microchip composite.
For solve the problems referred to above, the present invention by the following technical solutions:
A kind of preparation method of the graphene microchip composite printed for 3D, it is characterized in that: first graphite powder is added heat partition, the blade driven by the rotor of Type Impact Superfine Mill carries out shearing repeatedly, impact to graphite, make graphite pulverize to peel off, after classified screening, qualified material through electrostatic dispersion, obtain the number of plies 100 layers-300 layers be uniformly dispersed, the graphene microchip composite printed for 3D of good fluidity, concrete grammar is as follows:
(1) graphite powder and the dispersant that weight portion is 0.5-2.0 that weight portion is 90-100 are added heat partition in heated at high speed formula mixer, heated at high speed formula mixer rotating speed is 300-500rpm, heating-up temperature is 80-110 DEG C, and heating jitter time is 20-30min, obtains mixed material;
(2) mixed material step (1) obtained is sent into and is pulverized stripping in Type Impact Superfine Mill, and material enters the first pulverizing chamber under air-flow drives and pulverizes stripping for the first time;In the first pulverizing chamber, material is sheared, is impacted by revolution first order rotor banding cutting blade repeatedly at a high speed, crushing material is made to peel off, qualified thin material enters the second pulverizing chamber with air-flow, the defective rotated blanking device of thick material returns the first pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(3) qualified thin material enters the second pulverizing chamber fine crushing stripping further with air-flow;In the second pulverizing chamber, material is sheared, is impacted by revolution second level rotor banding cutting blade repeatedly at a high speed, the further fine crushing of material is made to peel off, sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan, the defective rotated blanking device of thick material returns the second pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(4), after sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan in step (3), by turbine bypass machine sizing screening, the number of plies uniform graphene microchip at 100-300 layer is obtained;
(5) the graphene microchip electrostatic dispersion that step (4) obtained processes, and is uniformly dispersed, the graphene microchip composite printed for 3D of good fluidity.
Described graphite powder is the one in expanded graphite, thermal cracking graphite, and particle diameter is between 1mm and 5mm.
Described dispersant is calgon, any one in sodium tripolyphosphate, lauryl sodium sulfate, polyacrylamide.
Described first order rotor speed is 3500-6000rpm.
The blade that described first order rotor drives is high hardness wear-resisting tooth profile metal cutter.
Described second level rotor speed is 5000-9000rpm.
The blade that described second level rotor drives is high hardness wear-resisting tooth profile metal cutter.
Described Type Impact Superfine Mill includes hopper, charger, casing, first order rotor, addendum cone, second level rotor, blocking material ring, fan, valve, deslagging spiral, the first pulverizing chamber, the second pulverizing chamber.First carry out adding dirt count in heated at high speed formula mixer by material, reduce Van der Waals force between graphite linings, making graphite linings be more easy to be stripped, then sent into by material in Type Impact Superfine Mill, material enters the first pulverizing chamber under air-flow drives and pulverizes stripping for the first time;In the first pulverizing chamber, material is sheared, is impacted by revolution first order rotor banding cutting blade repeatedly at a high speed, crushing material is made to peel off, qualified thin material enters the second pulverizing chamber with air-flow, the defective rotated blanking device of thick material returns the first pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;Qualified thin material enters the second pulverizing chamber fine crushing stripping further with air-flow;In the second pulverizing chamber, material is sheared, is impacted by the second level rotor banding cutting blade of higher rotating speed revolution further repeatedly, make materials fineization pulverize to peel off, obtain sheet high-specific surface area material, and the defective rotated blanking device of thick material returns the second pulverizing chamber and again pulverizes stripping, material is difficult to the particle pulverized and the impurity that is mixed into falls into deslagging spiral and is automatically drained out outside machine;Sheet high-specific surface area material sends into the further sizing screening of turbine bypass machine with air-flow and fan, then processes by electrostatic dispersion, obtain the number of plies be 100-300 layer be uniformly dispersed, the graphene microchip composite for 3D printing of good fluidity.
Although Graphene has the mechanical strength of excellence, conduction, heat conductivility, but reunite owing to Graphene can produce self, not only break up its scattered uniformity, compactness, and reduce mobility, it is applied to reunite when 3D prints, the internal stress that produces is concentrated, and not only may block printing head, mechanical strength, conduction, heat conductivility also can be caused to decline.In order to promote the extensive application of grapheme material, the present invention proposes the preparation method of a kind of graphene microchip composite printed for 3D, the method can the acquisition number of plies of volume production at being uniformly dispersed of 100-300 layer, the graphene microchip composite printed for 3D of good fluidity, production process is pollution-free, low energy consumption, concise in technology, and production cost is low;The graphene microchip not only number of plies of preparation uniformly, dispersiveness and good fluidity, and have the mechanical strength of excellence, conduction, heat conductivility concurrently, and good lubrication, high temperature resistant and anticorrosion properties, the graphene composite material of the present invention is used for 3D printing consumables, the mechanical strength of 3D printing consumables, conduction, heat conductivility will be significantly improved.
The preparation method of a kind of graphene microchip composite printed for 3D of the present invention, compared with prior art, its prominent feature and excellent effect are:
1, utilizing Type Impact Superfine Mill to shear, impact, successively twice classification grinding peels off graphite linings, it is ensured that the uniform quality of the graphene microchip composite printed for 3D obtained.
2, utilizing and add heat partition pretreating graphite, reduce Van der Waals force between graphite linings, make graphite linings more be easily peeled, the graphene microchip simultaneously prepared processes through electrostatic dispersion, makes the graphene composite material good fluidity of preparation, is uniformly dispersed, is difficult to reunite.
3, preparation method of the present invention is easily controllable, can realize the closed production of serialization, puts into little, low cost, non-environmental-pollution, yield height, has significant market using value.
Accompanying drawing explanation
For further illustrating the preparation method of a kind of graphene microchip composite printed for 3D, illustrated by accompanying drawing.
Accompanying drawing 1: for Type Impact Superfine Mill schematic diagram.1-hopper, 2-charger, 3-casing, 4-first order rotor, 5-addendum cone, 6-second level rotor, 7-blocking material ring, 8-fan, 9-valve, 10-deslagging spiral, 11-the first pulverizing chamber, 12-the second pulverizing chamber.
Detailed description of the invention
Below by way of detailed description of the invention, the present invention is described in further detail, but this should not being interpreted as, the scope of the present invention is only limitted to Examples below.In the case of without departing from said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change, should be included in the scope of the present invention.
Embodiment 1
A kind of preparation method of the graphene microchip composite printed for 3D:
(1) graphite powder and the dispersant that weight portion is 0.5 that weight portion is 90 being added in heated at high speed formula mixer heat partition, heated at high speed formula mixer rotating speed is 300rpm, and heating-up temperature is 80 DEG C, and heating jitter time is 20min, obtains mixed material;
(2) mixed material step (1) obtained is sent into and is pulverized stripping in Type Impact Superfine Mill, and material enters the first pulverizing chamber under air-flow drives and pulverizes stripping for the first time;In the first pulverizing chamber, material is sheared, is impacted by revolution first order rotor banding cutting blade repeatedly at a high speed, crushing material is made to peel off, qualified thin material enters the second pulverizing chamber with air-flow, the defective rotated blanking device of thick material returns the first pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(3) qualified thin material enters the second pulverizing chamber fine crushing stripping further with air-flow;In the second pulverizing chamber, material is sheared, is impacted by revolution second level rotor banding cutting blade repeatedly at a high speed, the further fine crushing of material is made to peel off, sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan, the defective rotated blanking device of thick material returns the second pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(4), after sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan in step (3), by turbine bypass machine sizing screening, the number of plies uniform graphene microchip at 100-300 layer is obtained;
(5) the graphene microchip electrostatic dispersion that step (4) obtained processes, and is uniformly dispersed, the graphene microchip composite printed for 3D of good fluidity.
Embodiment 2
A kind of preparation method of the graphene microchip composite printed for 3D:
(1) graphite powder and the dispersant that weight portion is 2.0 that weight portion is 100 being added in heated at high speed formula mixer heat partition, heated at high speed formula mixer rotating speed is 500rpm, and heating-up temperature is 110 DEG C, and heating jitter time is 30min, obtains mixed material;
(2) mixed material step (1) obtained is sent into and is pulverized stripping in Type Impact Superfine Mill, and material enters the first pulverizing chamber under air-flow drives and pulverizes stripping for the first time;In the first pulverizing chamber, material is sheared, is impacted by revolution first order rotor banding cutting blade repeatedly at a high speed, crushing material is made to peel off, qualified thin material enters the second pulverizing chamber with air-flow, the defective rotated blanking device of thick material returns the first pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(3) qualified thin material enters the second pulverizing chamber fine crushing stripping further with air-flow;In the second pulverizing chamber, material is sheared, is impacted by revolution second level rotor banding cutting blade repeatedly at a high speed, the further fine crushing of material is made to peel off, sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan, the defective rotated blanking device of thick material returns the second pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(4), after sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan in step (3), by turbine bypass machine sizing screening, the number of plies uniform graphene microchip at 100-300 layer is obtained;
(5) the graphene microchip electrostatic dispersion that step (4) obtained processes, and is uniformly dispersed, the graphene microchip composite printed for 3D of good fluidity.
Embodiment 3
A kind of preparation method of the graphene microchip composite printed for 3D:
(1) graphite powder and the dispersant that weight portion is 0.8 that weight portion is 91 being added in heated at high speed formula mixer heat partition, heated at high speed formula mixer rotating speed is 400rpm, and heating-up temperature is 90 DEG C, and heating jitter time is 25min, obtains mixed material;
(2) mixed material step (1) obtained is sent into and is pulverized stripping in Type Impact Superfine Mill, and material enters the first pulverizing chamber under air-flow drives and pulverizes stripping for the first time;In the first pulverizing chamber, material is sheared, is impacted by revolution first order rotor banding cutting blade repeatedly at a high speed, crushing material is made to peel off, qualified thin material enters the second pulverizing chamber with air-flow, the defective rotated blanking device of thick material returns the first pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(3) qualified thin material enters the second pulverizing chamber fine crushing stripping further with air-flow;In the second pulverizing chamber, material is sheared, is impacted by revolution second level rotor banding cutting blade repeatedly at a high speed, the further fine crushing of material is made to peel off, sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan, the defective rotated blanking device of thick material returns the second pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(4), after sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan in step (3), by turbine bypass machine sizing screening, the number of plies uniform graphene microchip at 100-300 layer is obtained;
(5) the graphene microchip electrostatic dispersion that step (4) obtained processes, and is uniformly dispersed, the graphene microchip composite printed for 3D of good fluidity.
Embodiment 4
A kind of preparation method of the graphene microchip composite printed for 3D:
(1) graphite powder and the dispersant that weight portion is 1.4 that weight portion is 96 being added in heated at high speed formula mixer heat partition, heated at high speed formula mixer rotating speed is 450rpm, and heating-up temperature is 100 DEG C, and heating jitter time is 20min, obtains mixed material;
(2) mixed material step (1) obtained is sent into and is pulverized stripping in Type Impact Superfine Mill, and material enters the first pulverizing chamber under air-flow drives and pulverizes stripping for the first time;In the first pulverizing chamber, material is sheared, is impacted by revolution first order rotor banding cutting blade repeatedly at a high speed, crushing material is made to peel off, qualified thin material enters the second pulverizing chamber with air-flow, the defective rotated blanking device of thick material returns the first pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(3) qualified thin material enters the second pulverizing chamber fine crushing stripping further with air-flow;In the second pulverizing chamber, material is sheared, is impacted by revolution second level rotor banding cutting blade repeatedly at a high speed, the further fine crushing of material is made to peel off, sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan, the defective rotated blanking device of thick material returns the second pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(4), after sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan in step (3), by turbine bypass machine sizing screening, the number of plies uniform graphene microchip at 100-300 layer is obtained;
(5) the graphene microchip electrostatic dispersion that step (4) obtained processes, and is uniformly dispersed, the graphene microchip composite printed for 3D of good fluidity.
Embodiment 5
A kind of preparation method of the graphene microchip composite printed for 3D:
(1) graphite powder and the dispersant that weight portion is 1.8 that weight portion is 95 being added in heated at high speed formula mixer heat partition, heated at high speed formula mixer rotating speed is 360rpm, and heating-up temperature is 85 DEG C, and heating jitter time is 30min, obtains mixed material;
(2) mixed material step (1) obtained is sent into and is pulverized stripping in Type Impact Superfine Mill, and material enters the first pulverizing chamber under air-flow drives and pulverizes stripping for the first time;In the first pulverizing chamber, material is sheared, is impacted by revolution first order rotor banding cutting blade repeatedly at a high speed, crushing material is made to peel off, qualified thin material enters the second pulverizing chamber with air-flow, the defective rotated blanking device of thick material returns the first pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(3) qualified thin material enters the second pulverizing chamber fine crushing stripping further with air-flow;In the second pulverizing chamber, material is sheared, is impacted by revolution second level rotor banding cutting blade repeatedly at a high speed, the further fine crushing of material is made to peel off, sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan, the defective rotated blanking device of thick material returns the second pulverizing chamber and again pulverizes stripping, and the particle being difficult to pulverize in material falls into deslagging spiral with the impurity being mixed into and is automatically drained out outside machine;
(4), after sheet high-specific surface area material sends into turbine bypass machine with air-flow and fan in step (3), by turbine bypass machine sizing screening, the number of plies uniform graphene microchip at 100-300 layer is obtained;
(5) the graphene microchip electrostatic dispersion that step (4) obtained processes, and is uniformly dispersed, the graphene microchip composite printed for 3D of good fluidity.